US6524714B1 - Heat treatable coated articles with metal nitride layer and methods of making same - Google Patents

Heat treatable coated articles with metal nitride layer and methods of making same Download PDF

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US6524714B1
US6524714B1 US09/847,663 US84766301A US6524714B1 US 6524714 B1 US6524714 B1 US 6524714B1 US 84766301 A US84766301 A US 84766301A US 6524714 B1 US6524714 B1 US 6524714B1
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Prior art keywords
coated article
layer
value
heat treatment
metal nitride
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US20030031879A1 (en
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George Neuman
Grzegorz Stachowiak
Hong Wang
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Guardian Glass LLC
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Guardian Industries Corp
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Assigned to GUARDIAN INDUSTRIES CORPORATION reassignment GUARDIAN INDUSTRIES CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: STACHOWIAK, GRZEGORZ, WANG, HONG, NEUMAN, GEORGE
Priority to EP02739204A priority patent/EP1448491A2/en
Priority to PCT/US2002/013597 priority patent/WO2002090281A2/en
Priority to PL367323A priority patent/PL204881B1/pl
Priority to CA002443742A priority patent/CA2443742C/en
Priority to US10/318,029 priority patent/US6716532B2/en
Priority to US10/353,088 priority patent/US20030180546A1/en
Publication of US20030031879A1 publication Critical patent/US20030031879A1/en
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Assigned to GUARDIAN GLASS, LLC. reassignment GUARDIAN GLASS, LLC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GUARDIAN INDUSTRIES CORP.
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12826—Group VIB metal-base component
    • Y10T428/12847—Cr-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12944—Ni-base component

Definitions

  • This invention relates to coated articles that have approximately the same color characteristics as viewed by the naked eye before and after heat treatment (e.g., thermal tempering), and corresponding methods.
  • Such coated articles may be used in insulating glass (IG) units, vehicle windows, and/or other suitable applications.
  • IG insulating glass
  • U.S. Pat. No. 5,688,585 discloses a solar control coated article including glass/Si 3 N 4 /NiCr/Si 3 N 4 , wherein matchability is achieved with a single layer system.
  • the NiCr layer be substantially free of any nitride.
  • An object of the '585 patent is to provide a sputter coated layer system that after heat treatment is matchable colorwise with its non-heat-treated counterpart.
  • the '585 patent uses a heat treatment (HT) of only three (3) minutes (col. 10, line 55).
  • this coated article has a rather high transmissive ⁇ E* value of about 5.9 after a heat treatment (HT) at 625 degrees C. for ten (10) minutes.
  • HT heat treatment
  • This high transmissive ⁇ E value means that a HT version of the '585 coated article does not approximately match colorwise non-heat-treated counterpart versions with regard to transmissive color after 10 minutes of HT. This is not desirable.
  • FIG. 15 is an XPS plot illustrating the Example 7 coating before heat treatment (HT), while FIG. 16 illustrates the Example 7 coating after HT.
  • FIG. 15 before heat treatment the three different layers are fairly separate and distinct.
  • the Ni slopes 3 on either side of the NiCr layer are very steep, as are the Si and N slopes 5 and 7 , respectively, on the lower side of the upper Si 3 N 4 layer. Therefore, the vast majority of the Ni is located in the NiCr layer and the vast majority of the Si and N from the upper Si 3 N 4 layer is located in that layer.
  • FIG. 15 is an XPS plot illustrating the Example 7 coating before heat treatment (HT)
  • FIG. 16 illustrates the Example 7 coating after HT.
  • the three different layers are fairly separate and distinct.
  • the Ni slopes 3 on either side of the NiCr layer are very steep, as are the Si and N slopes 5 and 7 , respectively, on the lower side of the upper Si 3 N 4 layer. Therefore, the vast majority of the Ni is located in the NiCr layer
  • FIG. 16 illustrates that when the FIG. 15 coated article of Example 7 is heat treated (HT) for 10 minutes as discussed above, a significant portion of the Ni from the NiCr layer migrates into the upper Si 3 N 4 layer. Additionally, upon HT a significant portion of the Si and N from the upper Si 3 N 4 layer migrates into the NiCr layer. In other words, the interface between the metal NiCr layer and the upper Si 3 N 4 layer becomes blurred and non-distinct. This is evidenced in FIG. 16 by the less steep slope 3 a of the Ni on the upper/outer side of the NiCr layer, and by the less steep slopes 5 a and 7 a of the Si and N on the lower side of the upper Si 3 N 4 layer. Still further, it can be seen by comparing FIGS. 15 and 16 that HT causes a significant amount of the Cr in the NiCr layer to migrate within that layer toward the upper side thereof so that it is not as uniformly distributed compared to pre-HT.
  • HT heat treated
  • An object of this invention is to provide a coating or layer system that has good color stability (i.e., a low ⁇ E* value(s)) with heat treatment (HT).
  • Another object of this invention is to provide a coating or layer system having a ⁇ E* value (transmissive and/or glass side reflective) no greater than 5.0 (more preferably no greater than 4.0, and most preferably no greater than 3.0) upon heat treatment (HT) at a temperature of at least about 600 degrees C. for a period of time of at least 5 minutes (more preferably at least 7 minutes, and most preferably at least 9 minutes).
  • a ⁇ E* value transmissive and/or glass side reflective
  • Another object of this invention is to nitride a Ni and/or Cr inclusive layer (e.g., a NiCr layer) to an extent so as to enable the resulting coated article to have the aforesaid low ⁇ E value(s).
  • a Ni and/or Cr inclusive layer e.g., a NiCr layer
  • Another object of this invention is to fulfill one or more of the above-listed objects.
  • certain example embodiments of this invention fulfill one or more of the above listed objects and/or needs by providing a coated article comprising:
  • a layer system supported by a glass substrate said layer system comprising a metal nitride inclusive layer located between first and second dielectric layers, wherein the second dielectric layer is at least partially nitrided and positioned so that the metal nitride inclusive layer is between the second dielectric layer and the glass substrate;
  • said coated article has a transmissive ⁇ E* T value no greater than 5.0 after at least about 5 minutes of heat treatment at a temperature(s) of at least about 600 degrees C.
  • Certain other example embodiments of this invention fulfill one or more of the above-listed objects and/or needs by providing a coated article comprising:
  • a layer system supported by a glass substrate said layer system comprising a metal nitride inclusive layer located between said glass substrate and an at least partially nitrided dielectric layer, wherein the metal nitride comprises at least one of NiN x and CrN x and contacts said dielectric layer;
  • coated article has a glass side reflective ⁇ E* G value no greater than 5.0 in view of thermal tempering including heat treating for at least about 5 minutes.
  • Certain other example embodiments of this invention fulfill one or more of the above-listed objects and/or needs by providing a coated article comprising:
  • a layer system supported by a glass substrate comprising a NiCrN x inclusive layer wherein at least 50% of the Cr is nitrided, said NiCrN x inclusive layer being located between and contacting first and second dielectric layers, wherein the second dielectric layer is at least partially nitrided and positioned so that the NiCrN x inclusive layer is between the second dielectric layer and the glass substrate;
  • said coated article has a transmissive ⁇ E* T value no greater than 5.0 following or due to heat treatment.
  • Still further example embodiments of this invention fulfill one or more of the above-listed objects and/or needs by providing a method of making a coated article, the method comprising:
  • a metal on the substrate in an atmosphere including a significant amount of nitrogen in order to form a metal nitride inclusive layer on the glass substrate;
  • a dielectric nitride inclusive layer on the substrate over the metal nitride inclusive layer;
  • the article which includes at least the metal nitride inclusive layer and the dielectric nitride inclusive layer for at least 5 minutes, the metal nitride inclusive layer being nitrided to an extent so that after said heat treating the article has a ⁇ E value of no greater than 5.0.
  • FIG. 1 is a partial side cross sectional view of an embodiment of a coated article (heat treated or not heat treated) according to an example embodiment of this invention.
  • FIG. 2 is a partial cross-sectional view of an IG unit as contemplated by this invention, in which the coating or layer system of FIG. 1 may be used.
  • FIG. 3 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 1 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time (i.e., the ⁇ depth is not actual depth, but instead is how deep into a reference SiO 2 layer sputtering would have reached over the corresponding time).
  • XPS x-ray photoelectron spectroscopy
  • FIG. 4 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 1 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 5 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 2 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 6 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 2 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 7 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 3 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 8 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 3 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 9 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 4 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 10 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 4 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 11 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 5 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 12 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 5 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 13 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 6 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 14 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 6 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 15 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 7 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 16 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 7 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 17 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 8 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 18 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 8 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 19 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 9 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 20 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 9 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • FIG. 21 is an x-ray photoelectron spectroscopy (XPS) graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of a layer system according to Example 10 of this invention (before heat treatment), where the “depth” axis refers to the depth into the coating and/or substrate from the exterior surface thereof as compared to the depth into a conventional SiO 2 layer that would have been achieved over the same period of time.
  • XPS x-ray photoelectron spectroscopy
  • FIG. 22 is an XPS graph illustrating the atomic % of components N, O, Na, Al, Si, Ca, Cr, and Ni throughout the thickness of the layer system according to Example 10 of this invention after heat treatment at 625 degrees C. for 10 minutes.
  • Certain embodiments of this invention provide a coating or layer system that may be used in applications such as IG units, vehicle windows, architectural windows, and/or other suitable applications. Certain embodiments of this invention provide a layer system that has excellent color stability (i.e., a low value of ⁇ E* and/or a low value of ⁇ a*; where ⁇ is indicative of change in view of HT) with heat treatment (e.g., thermal tempering, bending, or thermal heat strengthening) monolithically and/or in the context of dual pane environments such as IG units or windshields. Such heat treatments often necessitate heating the coated substrate to temperatures from about 600° C. up to about 800° C. for at least about 5 minutes.
  • heat treatment e.g., thermal tempering, bending, or thermal heat strengthening
  • FIG. 1 is a side cross sectional view of a coated article according to an example embodiment of this invention.
  • the coated article includes substrate 11 (e.g., clear, green, bronze, grey, blue, or blue-green glass substrate from about 1.0 to 12.0 mm thick), optional first dielectric layer 13 (e.g., of or including silicon nitride (e.g., Si 3 N 4 ), titanium dioxide, titanium nitride, zirconium nitride, silicon oxynitride, or the like), IR reflecting nickel (Ni) or nickel-chrome inclusive layer 15 that is nitrided (e.g., NiCrN x ), and second nitrided dielectric layer 17 (e.g., of or including silicon nitride (e.g., Si 3 N 4 ), titanium nitride, zirconium nitride, silicon oxynitride, aluminum nitride, or the like).
  • substrate 11 e.g.,
  • the coating system 19 includes metal nitride layer 15 located between (directly or indirectly) a pair of dielectric anti-reflection layers 13 and 17 .
  • Underlayer 13 is optional, and upper dielectric layer 17 is preferably at least partially nitrided.
  • coatings according to this invention can be made more color stable with heat treatment (HT) if layer 15 is nitrided during the deposition process (e.g., the layer is nitrided so as to be deposited as NiCrN x ). It is believed that by at least partially nitriding layer 15 during the deposition process (i.e., so that it is nitrided to some significant extent prior to HT), migration of N, Cr, and/or Ni can be reduced during HT thereby enabling the resulting coated article to be more color-stable with HT (i.e., have a lower ⁇ E* value(s)).
  • HT heat treatment
  • Metal in metal nitride layer 15 may or may not be fully nitrided in different embodiments of this invention.
  • metal such as Cr in layer 15 may be at least about 40% nitrided in certain embodiments of this invention, more preferably at least about 50% nitrided, even more preferably at least about 60% nitrided, and most preferably at least about 75% nitrided.
  • layer 15 is NiCrN x , it is believed that the layer includes at least Ni and CrN x .
  • layer 15 may be an oxynitride layer (e.g., a metal oxynitride).
  • metal nitride layer 15 may or may not include amounts of oxide in different embodiments of this invention.
  • dielectric anti-reflection layers 13 and 17 each have an index of refraction less than that of metal nitride layer 15 for anti-reflective purposes (e.g., silicon nitride layers 13 and 17 may have an index of refraction “n” of from about 1.9 to 2.1, while the metal nitride layer 19 has an index “n” higher than that).
  • the layer system 19 is “on” or “supported by” substrate 11 (directly or indirectly), other layer(s) may be provided therebetween.
  • the layer system 19 of FIG. 1 is considered “on” the substrate 11 even when other layer(s) are provided therebetween.
  • layers 13 and 17 comprise silicon nitride (e.g., Si 3 N 4 )
  • sputtering targets including Si employed to form these layers may be admixed with up to 6-20% by weight aluminum or stainless steel (e.g. SS#316), with about this amount then appearing in the layers so formed.
  • layer 15 may be NiCrN x , NiN x , or CrN x in certain embodiments of this invention, these materials are not limiting and other IR reflecting metal nitrides may instead be used.
  • any suitable ratio of Ni:Cr may be used.
  • the Ni:Cr ratio in this layer may be 50:50 in certain embodiments, may be 80:20 in other embodiments, and may be 90:10 or any other suitable ratio in still other embodiments.
  • FIG. 2 illustrates the coating or layer system 19 of FIG. 1 being utilized on surface # 2 of an IG (insulating glass) window unit.
  • IG insulating glass
  • the IG unit includes outside glass pane or sheet 11 and inside glass pane or sheet 23 .
  • These two glass substrates e.g., float glass 2 mm to 12 mm thick
  • a conventional sealant not shown
  • a conventional desiccant strip not shown
  • insulating space 25 may be at a pressure less than atmospheric pressure in certain alternative embodiments, although this of course is not necessary in all IG embodiments.
  • Coating 19 may be provided on the inner wall of substrate 11 in certain embodiments of this invention (as in FIG. 2 ), and/or on the inner wall of substrate 23 in other embodiments of this invention.
  • the preferred thicknesses and materials for the respective layers on the glass substrate 11 are as follows:
  • the color stability with lengthy HT due at least to the nitriding of layer 15 results in substantial matchability between heat-treated and non-heat treated versions of the coating or layer system.
  • two glass substrates having the same coating system thereon appear to the naked human eye to look substantially the same.
  • ⁇ E* and ⁇ a* are important in determining whether or not there is matchability, or substantial color matchability upon HT, in the context of this invention. Color herein is described by reference to the conventional a*, b* values. The term ⁇ a* is simply indicative of how much color value a* changes due to HT.
  • ⁇ E* (and ⁇ E) is well understood in the art and is reported, along with various techniques for determining it, in ASTM 2244-93 as well as being reported in Hunter et. al., The Measurement of Appearance , 2 nd Ed. Cptr. 9, page 162 et seq. [John Wiley & Sons, 1987].
  • ⁇ E* (and ⁇ E) is a way of adequately expressing the change (or lack thereof) in reflectance and/or transmittance (and thus color appearance, as well) in an article after or due to HT.
  • ⁇ E may be calculated by the “ab” technique, or by the Hunter technique (designated by employing a subscript “H”).
  • ⁇ E corresponds to the Hunter Lab L, a, b scale (or L h , a h , b h ).
  • ⁇ E* corresponds to the CIE LAB Scale L*, a*, b*. Both are deemed useful, and equivalent for the purposes of this invention.
  • CIE LAB 1976 the rectangular coordinate/scale technique known as the L*, a*, b* scale may be used, wherein:
  • a* is (CIE 1976) red-green units
  • ⁇ E may be calculated using equation (1) by replacing a*, b*, L* with Hunter Lab values a h , b h , L h . Also within the scope of this invention and the quantification of ⁇ E* are the equivalent numbers if converted to those calculated by any other technique employing the same concept of ⁇ E* as defined above.
  • coatings or layer systems herein provided on clear monolithic glass substrates have reflective color as follows before heat treatment, as viewed from the glass side of the coated article (R G %):
  • coatings or layer systems herein provided on clear monolithic glass substrates have transmissive color as follows before heat treatment:
  • layer systems-provided on clear monolithic glass substrates have color characteristics ⁇ E*, and ⁇ a*, and ⁇ b* as follows, when viewed from the glass (G) side (as opposed to the layer side) of the coated article:
  • transmissive color characteristics after HT in certain embodiments of this invention layer systems provided on clear monolithic glass substrates have transmissive color characteristics ⁇ E*, ⁇ a* and ⁇ b* as follows:
  • coated articles according to certain embodiments of this invention have a ⁇ E* G value (glass side) of no greater than 5.0, more preferably no greater than 4.0, and even more preferably no greater than 3.0; and have a ⁇ a* G value (glass side) of no greater than about 1.0, more preferably no greater than 0.6 and most preferably no greater than 0.3.
  • coated articles according to certain embodiments of this invention have a ⁇ E* T value (transmissive) of no greater than 5.0, more preferably no greater than 4.0, and even more preferably no greater than 3.0; and have a ⁇ a* T value (transmissive) of no greater than about 1.3, more preferably no greater than 1.1, and most preferably no greater than 0.8. When one or more of these are achieved, matchability may result.
  • Example coated articles each ultimately annealed and heat treated were made, with Examples 1-6 and 8-10 being made in accordance with certain example embodiments of this invention and Example 7 being made for purposes of comparison where the NiCr layer was not nitrided.
  • the layer system on about 6.0 mm thick clear soda-lime-silica glass substrate was: silicon nitride/NiCrN x ,/silicon nitride (e.g., see FIG. 1 ).
  • the layer system on about 6.0 mm thick clear soda-lime-silica glass substrate was: silicon nitride/NiCr/silicon nitride (i.e., the NiCr layer was not nitrided in comparative Ex. 7).
  • the coater/process setups for the Examples were as follows.
  • a Leybold Terra-G six-chamber sputter coating apparatus was used to sputter the coatings onto the glass substrates.
  • Five cathodes were in each chamber, so there were a total of 30 cathode targets in the sputter coater (not all were used).
  • Cathode numbering utilizes the first digit to refer to the coater chamber, and the second digit to refer to the cathode position in that chamber.
  • cathode # 42 was the second cathode (second digit) in the fourth (first digit) sputter chamber.
  • Cathode #s 42 , 55 and 61 were dual C-Mag type cathodes; and cathode #s 44 and 45 were planar cathodes.
  • C% refers to the percentage (%) of trim gas introduced at the center
  • PS% refers to the percentage of the trim gas introduced at the pump side
  • VS% refers to the percentage of the trim or tuning gas introduced at the viewer side.
  • the NiCr targets were approximately 80/20 NiCr.
  • Examples 1-6 and 8-10 were all deposited on respective glass substrates in a manner so that layer 15 (i.e., the NiCrN x ) layer was nitrided as deposited (due to intentional introduction of N gas into the sputter chamber including cathode(s) #s 44 and 45 ).
  • layer 15 i.e., the NiCrN x
  • Example 7 layer 15 (NiCr) was not nitrided, in order to illustrate the benefits of nitriding layer 15 according to this invention.
  • Examples 1-6 and 8-10 illustrate that layer 15 can be nitrided (via cathodes/targets 44-45) to various degrees (i.e., the nitrogen (N) flow ranged from 31 sccm in Example 6 up to about 230 sccm in Example 4). It will be shown below that each of these had better characteristics with regard to color stability upon HT than comparative Example 7 where no nitriding was done to the NiCr layer. Generally, the more nitriding of layer 15 , the lower the ⁇ E value and thus the better the color stability upon HT. Moreover, it can be seen that Examples 9-10 each had a Si-rich overcoat silicon nitride layer relative to the other Examples.
  • Examples 8-10 show the effect of N gas flow (mL/kW) on coating stability; e.g., the higher the N gas flow, the less Ni migration and more color stability with HT.
  • N gas flow mL/kW
  • Si-rich overcoat silicon nitride layers 17 are appropriate according to certain embodiments of this invention, it will be shown below that the Si-rich nature of the overcoat 17 tends to cause sheet resistance (R s ) to increase upon HT which is sometimes not desirable.
  • R s sheet resistance
  • Examples 1-10 were tested and were found to have the following characteristics monolithically (not in an IG unit), where the heat treatment (HT) involved heating the respective monolithic products at about 625 degrees C. for about 10 minutes. It is noted that a* and b* color coordinate values are in accordance with CIE LAB 1976, Ill. C 2 degree observer technique, ⁇ a* and ⁇ b* are in terms of absolute value. Moreover, sheet resistance (R s ) is in units of ohms per square as is known in the art.
  • each of Examples 1-6 and 8-10 had good matchability (i.e., transmissive and/or glass side reflective ⁇ E* no greater than 5.0) because layer 15 was nitrided.
  • ⁇ E T was very high in Ex. 7 at 5.9.
  • ⁇ E* was no greater than 5.0, more preferably no greater than 4.0 and in certain most preferred instances no greater than 3.0.
  • Example 7 experienced a very high ⁇ a* value of 1.53.
  • nitriding of layer 15 enables the resulting coated article to have much improved color stability upon lengthy HT (e.g., HT of at least 5 minutes).
  • FIGS. 3-4 are XPS plots of Example 1, before and after HT, respectively.
  • FIGS. 5-6 are XPS plots of Example 2 before and after HT, respectively;
  • FIGS. 7-8 are XPS plots of Example 3 before and after HT, respectively;
  • FIGS. 9-10 are XPS plots of Example 4 before and after HT, respectively;
  • FIGS. 11-12 are XPS plots of Example 5 before and after HT, respectively;
  • FIGS. 13-14 are XPS plots of Example 6 before and after HT, respectively;
  • FIGS. 15-16 are XPS plots of Example 7 before and after HT, respectively;
  • FIGS. 17-18 are XPS plots of Example 8 before and after HT, respectively;
  • FIGS. 19-20 are XPS plots of Example 9 before and after HT, respectively; and FIGS. 21-22 are XPS plots of Example 10 before and after HT, respectively.
  • N nitrogen
  • the nitrogen (N) signals reported in these Figures are taken from the 1s orbital of N as shown, and so forth. It is noted that the interface of the coating system with the underlying glass substrate can be seen in these FIGS. where Ca and Na begin to rise (e.g., around 750 ⁇ in FIGS. 3 - 4 ).
  • layer 17 may be a Si-rich form of silicon nitride in certain embodiments of this invention, this may cause significant Ni migration thereby causing sheet resistance to rise upon HT as shown in Example 10 (note the less steep Ni slope 3 a in FIG. 22, and the increase in R s , upon HT in Table 5).
  • N nitrogen
  • coated articles have a sheet resistance (R s ) of no greater than 500 ohms/sq. after HT, more preferably no greater than 250 ohms/sq. after HT, even more preferably no greater than about 100 ohms/sq., and most preferably no greater than about 41 ohms/sq. after HT.
  • coated articles herein experience a reduction in sheet resistance upon HT (in contrast to Example 7).
  • Coated articles herein in certain example embodiments also have a hemispherical emissivity (E h ) of no greater than about 1.0, more preferably no greater than about 0.5, and most preferably no greater than about 0.4 before and/or after HT.
  • E h hemispherical emissivity
  • nitriding layer 15 results in a more mechanically durable (e.g., scratch resistant) coated article after HT. This is believed to be because or the chrome nitride present in layer 15 .
  • Coated articles of certain embodiments of this invention are both chemically and mechanically durable.
  • monolithic coated articles according to certain embodiments of this invention preferably have a visible transmittance (TY%) of from 5-80% (more preferably from 7-20%) before and/or after HT.
  • monolithic coated articles according to certain embodiments of this invention preferably have a glass side reflectance value (R G Y %) of at least 15%, and more preferably from 20-42% before and/or after HT.
  • Examples 1-6 and 8-10 may ultimately be utilized in the context of an IG unit, a vehicle window, or the like.
  • Certain terms are prevalently used in the glass coating art, particularly when defining the properties and solar management characteristics of coated glass.
  • Intensity of reflected visible wavelength light i.e. “reflectance” is defined by its percentage and is reported as R x Y (i.e. the Y value cited below in ASTM E-308-85), wherein “X” is either “G” for glass side or “F” for film side.
  • Glass side e.g. “G”
  • film side i.e. “F”
  • Color characteristics are measured and reported herein using the CIE LAB a*, b* coordinates and scale (i.e. the CIE a*b* diagram, Ill. CIE-C, 2 degree observer). Other similar coordinates may be equivalently used such as by the subscript “h” to signify the conventional use of the Hunter Lab Scale, or Ill. CIE-C, 10° observer, or the CIE LUV u*v* coordinates.
  • These scales are defined herein according to ASTM D-2244-93 “Standard Test Method for Calculation of Color Differences From Instrumentally Measured Color Coordinates” Sep. 15, 1993 as augmented by ASTM E-308-85, Annual Book of ASTM Standards, Vol. 06.01 “Standard Method for Computing the Colors of Objects by 10 Using the CIE System” and/or as reported in IES LIGHTING HANDBOOK 1981 Reference Volume.
  • the term “transmittance” means solar transmittance, which is made up of visible light transmittance (TY), infrared radiation transmittance, and ultraviolet radiation transmittance. Total solar energy transmittance (TS) is then usually characterized as a weighted average of these other values.
  • visible transmittance (TY) is characterized by the standard CIE Illuminant C, 2 degree observer, technique at 380-720 nm; near-infrared is 720-2500 nm; ultraviolet is 300-800 nm; and total solar is 300-2500 nm.
  • a particular infrared range i.e. 2,500-40,000 nm is employed.
  • Visible transmittance can be measured using known, conventional techniques. For example, by using a spectrophotometer, such as a Perkin Elmer Lambda 900 or Hitachi U4001, a spectral curve of transmission is obtained. Visible transmission is then calculated using the aforesaid ASTM 308/2244-93 methodology. A lesser number of wavelength points may be employed than prescribed, if desired.
  • Another technique for measuring visible transmittance is to employ a spectrometer such as a commercially available Spectrogard spectrophotometer manufactured by Pacific Scientific Corporation. This device measures and reports visible transmittance directly. As reported and measured herein, visible transmittance (i.e. the Y value in the CIE tristimulus system, ASTM E-308-85) uses the Ill. C.,2 degree observer.
  • E is a measure, or characteristic of both absorption and reflectance of light at given wavelengths. When transmittance is zero, which is approximately the case for float glass with wavelengths longer than 2500 nm, the emittance may be represented by the formula:
  • emittance values become quite important in the so-called “mid-range”, sometimes also called the “far range” of the infrared spectrum, i.e. about 2,500-40,000 nm., for example, as specified by the WINDOW 4.1 program, LBL-35298 (1994) by Lawrence Berkeley Laboratories, as referenced below.
  • the term “emittance” as used herein, is thus used to refer to emittance values measured in this infrared range as specified by ASTM Standard E 1585-93 for measuring infrared energy to calculate emittance, entitled “Standard Test Method for Measuring and Calculating Emittance of Architectural Flat Glass Products Using Radiometric Measurements”. This Standard, and its provisions, are incorporated herein by reference.
  • emittance is reported as hemispherical emittance (E h ) and normal emittance (E n ).
  • E h hemispherical emittance
  • E n normal emittance
  • the actual accumulation of data for measurement of such emittance values is conventional and may be done by using, for example, a Beckman Model 4260 spectrophotometer with “VW” attachment (Beckman Scientific Inst. Corp.). This spectrophotometer measures reflectance versus wavelength, and from this, emittance is calculated using the aforesaid ASTM E 1585-93 which has been incorporated herein by reference.
  • Sheet resistance is a well known term in the art and is used herein in accordance with its well known meaning. It is here reported in ohms per square units. Generally speaking, this term refers to the resistance in ohms for any square of a layer system on a glass substrate to an electric current passed through the layer system. Sheet resistance is an indication of how well the layer or layer system is reflecting infrared energy, and is thus often used along with emittance as a measure of this characteristic. “Sheet resistance” may for example be conveniently measured by using a 4-point probe ohmmeter, such as a dispensable 4-point resistivity probe with a Magnetron Instruments Corp. head, Model M-800 produced by Signatone Corp. of Santa Clara, Calif.
  • Chemical durability or “chemically durable” is used herein synonymously with the term of art “chemically resistant” or “chemical stability”. Chemical durability is determined by boiling a 2′′ ⁇ 5′′ sample of a coated glass substrate in about 500 cc of 5% HCl for one hour (i.e. at about 220° F.). The sample is deemed to pass this test (and thus the layer system is “chemically resistant” or is deemed to be “chemically durable” or to have “chemical durability”) if the sample's layer system shows no visible discoloration or visible peeling, and no pinholes greater than about 0.003′′ in diameter after this one hour boil.
  • “Mechanical durability” as used herein is defined by the following tests.
  • the test uses a Pacific Scientific Abrasion Tester (or equivalent) wherein a 2′′ ⁇ 4′′ ⁇ 1′′ nylon brush is cyclically passed over the layer system in 500 cycles employing 150 gm of weight, applied to a 6′′ ⁇ 17′′ sample.
  • the test is deemed passed, and the article is said to be “mechanically durable” or to have “mechanical durability”.
  • heat treatment and “heat treating” as used herein mean heating the article to a temperature sufficient to enabling thermal tempering, bending, or heat strengthening of the glass inclusive article. This definition includes, for example, heating a coated article to a temperature of at least about 600 degrees C. for a sufficient period to enable tempering.

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PCT/US2002/013597 WO2002090281A2 (en) 2001-05-03 2002-05-02 Heat treatable coated articles with metal nitride layer and methods of making same
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CA002443742A CA2443742C (en) 2001-05-03 2002-05-02 Heat treatable coated articles with metal nitride layer and methods of making same
US10/318,029 US6716532B2 (en) 2001-05-03 2002-12-13 Heat treatable coated articles with metal nitride layer and methods of making same
US10/353,088 US20030180546A1 (en) 2001-05-03 2003-01-29 Heat treatable coated article with chromium nitride IR reflecting layer and method of making same
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CA2443742A1 (en) 2002-11-14
US20030108779A1 (en) 2003-06-12
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US20030031879A1 (en) 2003-02-13
US6926967B2 (en) 2005-08-09
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US20040161616A1 (en) 2004-08-19
WO2002090281A3 (en) 2004-06-17
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CA2443742C (en) 2009-09-29
US6716532B2 (en) 2004-04-06

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